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目的:建立测定血浆中尼美舒利(Nim)的反相高效液相色谱法。方法:血浆样品用甲醇沉淀蛋白,经酸化后加甲苯提取,氮气挥干,加流动相溶解进样。以YWGC18柱,甲醇0.05mol·L-1磷酸二氢钾(55∶45)为流动相,pH5.02,甲苯磺丁脲为内标,在波长230nm处检测。结果:在0.26μg·ml-1~10.8μg·ml-1浓度范围内,峰面积比与浓度呈良好线性关系,r=0.9995。最低检测限为0.2μg·ml-1,方法重现性好,方法回收率为86.0%~92.2%,萃取回收率为72.2%~88.4%。结论:用本方法测定8例单剂量po100mgNim的血药浓度,结果满意。
Objective: To establish a reversed-phase high performance liquid chromatography (HPLC) method for the determination of nimesulide in plasma. Methods: The plasma samples were precipitated with methanol, acidified and extracted with toluene, evaporated to dryness under nitrogen and dissolved in mobile phase. To YWG C18 column, methanol 0.05mol·L-1 potassium dihydrogen phosphate (55:45) as the mobile phase, pH5.02, tolbutamide as internal standard, at a wavelength of 230nm at the detection. Results: In the concentration range of 0.26μg · ml-1 ~ 10.8μg · ml-1, the peak area ratio showed a good linear relationship with the concentration, r = 0.9995. The detection limit was 0.2μg · ml-1. The method was reproducible. The recoveries were 86.0% -92.2%. The extraction recoveries were 72.2% -88.4%. Conclusion: This method was used to determine the blood concentration of eight single-dose po100mgNim, with satisfactory results.